基于UPLC-Q/TOF-MS技术的蒙药黑云香成分分析及HPLC含量测定研究

其其格; 包晓玲; 李淑艳; 乌日吉木斯; 韩阿斯如; 吴东兴

doi:10.13748/j.cnki.issn1007-7693.20241875

基于UPLC-Q/TOF-MS技术的蒙药黑云香成分分析及HPLC含量测定研究

Composition Analysis and HPLC Content Determination of Mongolian Medicine Commiphora Mukul (Hook. ex Stocks) Engl Based on UPLC-Q/TOF-MS

摘要

摘要:
目的基于UPLC-Q/TOF-MS技术分析蒙药黑云香成分，并采用HPLC同时测定黑云香中2种成分含量。
方法 UPLC-Q/TOF-MS法采用Waters acquity UPLC BEH C₁₈色谱柱(2.1 mm×100 mm，1.7 µm)，柱温35 ℃，流动相为甲醇(A)-0.1%甲酸水(B)，梯度洗脱；体积流量0.3 mL·min⁻¹；电喷雾离子源，正离子模式下采集质谱数据，质量扫描范围m/z 100~1000。使用UNIFI Portal 软件进行成分分析。HPLC使用Waters SymmetryR C₁₈色谱柱(4.6 mm×250 mm，5 μm)；流动相为甲醇(A)-0.1%磷酸水(B)，梯度洗脱；体积流量1.0 mL·min⁻¹；检测波长252 nm；柱温25 ℃。同时测定黑云香中2-甲氧基-5-乙酰基-呋喃吉玛(10)-烯-6-酮和脱氢松香酸2种成分的含量。
结果基于UPLC-Q/TOF-MS技术在正离子模式下检测出42个化合物；通过化合物的保留时间、母离子、碎片离子等相关信息，并查阅没药属药材的分离等相关文献，初步推测出化合物名称。采用HPLC进行2种成分的含量测定，分别在0.12~0.74、0.04~0.24 μg·mL⁻¹内线性关系良好(r>0.9991)，平均加样回收率分别为99.01%、99.46%，RSD分别为0.62%、0.66%。
结论采用UPLC-Q/TOF-MS技术可以快速、准确分析黑云香化学成分；建立的含量测定方法简便可靠，可用于黑云香质量控制。

Abstract:
OBJECTIVE To analyze the components of Commiphora mukul(Hook. ex Stocks) Engl based on the UPLC-Q/TOF-MS technique, and to simultaneous determine two components in it by HPLC.
METHODS The UPLC-Q/TOF-MS method was performed on Waters acquity UPLC BEH C₁₈ column(2.1 mm×100 mm, 1.7 µm), temperature was maitained at 35 ℃, using methanol(A)-0.1% formic acid water(B) as the mobile phase, gradient elution was performed. Volume flow rate was 0.3 mL·min⁻¹. Electrospray ionization(ESI) source was used to acquire mass spectrometry data in positive ion mode with the mass scanning range m/z 100−1000. The UNIFI Portal software was used for component analysis. Waters SymmetryR C₁₈ column(4.6 mm×250 mm, 5 μm) was used for HPLC. The mobile phase was methanol(A)-0.1% phosphoric acid water(B). Volume flow rate was 1.0 mL·min⁻¹. The detection wavelength was 252 nm. Column temperature was 25 ℃. At the same time, the contents of 2-methoxy-5-acetoxy-furanogermacr-1(10)-en-6-one and dehydroabietic acid were determined.
RESULTS Based on the UPLC-Q/TOF-MS technique, 42 compounds were detected in positive ion modes. The name of the compound was preliminarily inferred through the information of retention time, parent ion, fragment ion and related literature on the separation of myrrh. The contents of the two components were determined by HPLC, and the linear relationships were good(r>0.9991) in the range of 0.12−0.74 μg·mL⁻¹ and 0.04−0.24 μg·mL⁻¹. The average recoveries were 99.01% and 99.46%, and RSD were 0.62% and 0.66%.
CONCLUSION The UPLC-Q/TOF-MS technique can be used to analyze the chemical components of the Commiphora mukul(Hook. ex Stocks) Engl rapidly and accurately. The established content determination method is simple and reliable, and can be used for the quality control of Commiphora mukul(Hook. ex Stocks) Engl.

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